Process of producing dyeings fast to light



Patented .Dec.- 11, 1928.

UNITED STATES PATENT OFFICE.

PAUL BABE, HEBMANN STCTTER, AND BERTHOLD WENK, F IiEVERKUSEN-ON-THE- RHIHE, AND WILHELM SCHEPSS, OF WIESDORF-ON-THE-RHINE, GERMANY, AS- SIGNORS T0 GRASSELLI DYESTUFF CORPORATION, OF NEW YORK, N. Y., A COB- roaa'rron' or DELAWARE.

PROCESS OF PRODUCING DYEINGS FAST TO LIGHT.

No Drawing. Application filed December 15, 1926, Serial No. 155,101, and in Germany December 22, 1925.

This invention relates to a process for making dyeings of acid and basic dyestuffs on fibers whichare fast to light.

We have found that this can be accomplished by precipitating complex compounds of tungstic acids or 'molybdic acids or tungstic-molybdic acids or mixtures thereof and especially the phospho-tungstic acids, the

' phospho-molybdic acids, and the phosphotungstic-molybdic acids upon the fiber by means of organic fixators preliminary to the dyeing thereof with acid or basic dyestufi's.

By organic fixators we mean organic ma- I terials such as aliphatic and aromatic amines and their derivatives, phenols and their derivatives, thio-compounds and compounds having an alcoholic residue. The use of tannin as an organic fixator is excluded.

The so treated fibers are now able to take up acid and basic dyestufis giving dyeing having a particularly enhanced fastness to light as compared with similar .dyeings made by using tannin in place of the organic fixators referred to. I

We have found, further, that the lightfastness property of dyeings of acid and basic dyestufls may be enhanced by treating the said com lex compounds precipitated on the fiber wit reducing a ents, forexample, the I commonly used bisul tes, hydrosulfites, formaldehyde or the like.

In this case it is possible also to omit the treatment of the fibers with the so-called or ganic fixators since the treatment of complex tungstic acid and molybdic acid compounds upon the fiber with the said reducing agents effects the fixation thereof.

After-treatment of mordanted dyein'gs obtained according to this process with salts or acids, in the well known manner, for example,

with copper acetate, phospho-tungstic-molyo dic acid, or the like, may be resorted to, effecting'an enhanced fastness to washing.

' Example 1.

ton is then dyed, in the customary manner, with the dyestuft' obtainable from tetralnethyldlaminobenzhydrol and dibenzylanh linedisulfo acid. There is obtained thereby acid above-mentioned, there may be used phsispho-tungstic acid or phospho-molybdic aci Example 2.

Cotton is treated as described in Example 1 above, substituting phenol in place of the benzidine hydrochloride as the fixator. There is obtained, by dyeing the fiber so treated with the dyestufi' obtainable from ethyl-benzyl-mtoluidine sulfo acid and p-diethylaminobenzaldehyde, a blue dyeing that is characterized by an outstanding fastness to light ascon trastcdwith the basic blues obtainable on tannin-mordanted cotton:

Analogous results are obtained by substi- I tuting, for phenol itself, 1.8-dihydroxynaphthalene-3.6- disulfo acid or o'ther phenols such as thio-phenol.

Eocample 3.

Cotton is treated as described in the preceding examples, with the substitution of tetramethyldiaminobenzhydrolsulfo acid (Ber. 27, 1405) as fixator. The treated cotton is dyed with the dyestufi' disclosed in Germanpatent No. 287,003, yielding a greenish blue dyeing, of great fastness to light.

Example .4.

Acetate silk is treated with dibenzylanilinem-sulfoacid as fixator. Dyeing with the dyestuffs obtainable from tetramethyldiazninobenzhydrol nd ethylbenzyl-m-toluidinesulfo acid yields a yeing of an intense violet shade possessing great fastness to light. v

' E azample 5.

Cotton is treated as hereinbefore described with the exception that, in place of the previously mentioned fixators there is subgreat fastness to light.

stituted ra. su ar. U on d ein with the dyestufi' rlieiii one l in Ex zimplgz, a light blue dyeing is obtained which is characterized by a great fastness to light as contrasted to analogous dyeings on ta1min-mordanted cotton. In place of grape sugar may be used dextrine, starch, cane sugar, milk sugar or the like. With similar results one may use cyclohexanol and the like.

The washing-fastness of the dyeings obtained according to Examples 15 may be still further improved by after-treatment with salts or acids in the known manner, for example, with copper acetate, phospho-tungstic-molybdic acid or the like.

Example 6.

The fiber, treated as described in Example 5, is dyed with China green (Schulz-Julius, 1914, 495), yielding a clear green dyeing of Example 7.

Cotton is padded with a 1% solution of phospho-tungstic-molybdic acid, squeezed out, and treated with a solution of sodium bisulfite and sulfuric acid; rinsed, and, in the ordinary manner, dyed with 1% China green crystals or other basic dyestuif.

We claim:

1. In the process of dyeing fiber the step which comprises precipitating on the fiber by means of an organic fixator a complex acid containing at least one metal of the group including molybdenum and tungsten.

2. In the process of dyeing fiber the step which comprises precipitating on the fiber by means of an organic fixator a complex phosphoric acid containing at least one metal of the group including molybdenum and tungsten.

3. In the process of dyeing fiber the step which comprises precipitating on the fiber by means of an organic fixator a complex phosphoric acid containing tungsten.

4. In the process of dyeing fiber the step which comprises precipitating on the fiben by means of an organic fixator a complex phospho-tungstic-molybdic acid.

5. The process of dyeing fiber which comprises precipitating on the fiber by means of an organic fixator a complex acid containing at least one metal of the group 'includipg molybdenum and tungsten and then dyeing the fiber by means ofa dyestuif of the group including the acid and basic dyestuffs 6. The process of dyeing fiber which comprises preci itating on the fiber by means of an organic xator a complex phosphoric acid containing at least one metal of the group including molybdenum and tungsten and then dyeing, the fiber by means of a d estufl of the group including the acid an basic dyestuffs.

7. The process of dyeing fiber which comprises precipitating on the fiber by means of an organic fixator a complex phosphoric acid containing tungsten and then dyeing the fiber by means of a dyestufi of the group including the acid and basic dyestuils.

8. The process of dyeing fiber which comprises precipitating on the fiber by means of an organic fixator a complex phospho-tungstic-molybdic acid and then dyeing the fiber by means of a dyestufl of the group including the acid and basic dyestuffs.

9. The process of dyeing which comprises precipitating on the fiber by means of an organic fixator a complex acid containing at least one metal of the group including molybdenum and tungsten, treating the precipi- V tated compound on the fiber with a reducing agent and dyeing the fiber by means of a dyestufli of the group including the acid and basic dyestuffs.

10. The process of dyeing which comprises precipitating on the fiber bymeans of an organic fixator a complex phosphoric acid containing atleast one metal of the group including molybdenum and tungsten, treating the precipitated .compound on the fiber with a reducing agent and dyeing the fiber by means of a dyestufi of the group including the acid and basic dyestuffs. I

11. The process of dyeing which comprises precipitating on the fiber by means of an organic fixator a complex phosphoric acid containing tungsten, treating the precipitated-compound on the fiber with a reducing agent and dyeing the fiber by means of a dyestufi of the group including the acid and basic dyestuffs.

precipitating on the fiber by means of an organic fixator a complex phospho-tungstic molybdic acid, treating the precipitated compound on the fiber with a reducing agent and dyeing the fiber by means of a dyestufi of the group including the acid and basic dyestufls.

13. The process of dyeing fiber which comprises precipitating on the fiber by means of an aromatic phenoliccompound containing not more than three phenolic OH groups, a complex phosphoric acid containing at least one metal of the group including molybdenum and tungsten, and then dyeing the fiber by means of a dyestufif of the group including the acid and basic dyestuffs.

14. The process of dyeing fiber which comprises precipitating on the fiber by means of an aromatic phenolic compound containing not more than three phenolic OH groups, a complex. phospho-tungstic-molybdic acid, and then dyeing the fiber by means of a dyestuff of the group including the acid and prises precipitating on the fiber by means of phenol a complex phosphoric acid contain- 12. The process of dyeing which comprises I ing at least one metal of the group including a dyestufi of the group including the acid molybdenum and tungsten, and then dyeing :and basic dyestuffs. 10

In testimony whereof, we aflix our slgnathe fiber by means of a dyestufi' of the group including the acid and basic dyestuffs.

16. The process of dyeing fiber which comtures.

prises precipitating on the fiber by means of phenol a complex phospho-tungstic-molybdic acid, and then dyeing the fiber by means of PAUL RABE. HERMANN STOTTER. BERTHOLD WENK. WILHELM SCHEPSS. 

